CN114146685A - Nickel-based purifying agent and preparation method and application thereof - Google Patents
Nickel-based purifying agent and preparation method and application thereof Download PDFInfo
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- CN114146685A CN114146685A CN202111497639.1A CN202111497639A CN114146685A CN 114146685 A CN114146685 A CN 114146685A CN 202111497639 A CN202111497639 A CN 202111497639A CN 114146685 A CN114146685 A CN 114146685A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 239000012629 purifying agent Substances 0.000 title claims abstract description 64
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 84
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 31
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 31
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000001556 precipitation Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 10
- 150000002815 nickel Chemical class 0.000 claims abstract description 7
- 239000012716 precipitator Substances 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 7
- -1 rare earth metal salt Chemical class 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000011261 inert gas Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 14
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 13
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 12
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 229910001954 samarium oxide Inorganic materials 0.000 claims description 10
- 229940075630 samarium oxide Drugs 0.000 claims description 10
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 10
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000003245 coal Substances 0.000 claims description 6
- YZDZYSPAJSPJQJ-UHFFFAOYSA-N samarium(3+);trinitrate Chemical compound [Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZDZYSPAJSPJQJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 2
- 244000060011 Cocos nucifera Species 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims description 2
- 229910003447 praseodymium oxide Inorganic materials 0.000 claims description 2
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002516 radical scavenger Substances 0.000 claims 7
- 230000000274 adsorptive effect Effects 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 26
- 239000007789 gas Substances 0.000 abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- 238000000746 purification Methods 0.000 abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 238000013329 compounding Methods 0.000 abstract description 3
- 238000006356 dehydrogenation reaction Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 16
- 239000002244 precipitate Substances 0.000 description 9
- 238000000227 grinding Methods 0.000 description 8
- 238000007873 sieving Methods 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
- B01D2257/108—Hydrogen
Abstract
The invention belongs to the field of gas purification, and particularly relates to a nickel-based purifying agent as well as a preparation method and application thereof. The nickel-based purifying agent comprises the following components in percentage by mass: 75-85 wt% of nickel oxide, 5-15 wt% of aluminum oxide, 1-5 wt% of rare earth metal oxide and 5-15 wt% of active carbon. Adding nickel salt and rare earth metal salt into deionized water for dissolving, adding an alumina precursor to obtain a mixed material, adding activated carbon into the mixed material, adding a precipitator for reaction to generate a precipitation product, performing suction filtration, washing, drying and roasting on the precipitation product to obtain a mixture of nickel oxide, alumina, rare earth metal oxide and activated carbon, and performing tabletting molding to obtain the nickel-based purifying agent. The nickel-based purifying agent is used for adsorbing and removing hydrogen in inert gas, the purifying agent comprises nickel oxide, aluminum oxide, rare earth metal oxide and active carbon, and multiple components act synergistically, the purifying agent obtained by compounding is used for adsorbing and removing hydrogen in nitrogen, and the nickel-based purifying agent has the characteristics of high hydrogen adsorption capacity, high dehydrogenation precision, long service life, capability of being repeatedly regenerated and used, simple preparation process, low cost and good industrial application prospect.
Description
Technical Field
The invention belongs to the field of gas purification, and particularly relates to a nickel-based purifying agent as well as a preparation method and application thereof.
Background
An ultrapure gas refers to a gas having a purity of greater than 99.99%. Ultrapure gases are mostly purified from industrial gases, and include adsorption, absorption, electrolysis, cryogenic rectification, and catalysis. With the development of semiconductor devices, especially large scale integrated circuits, the market demand for ultra-pure gases is increasing, and therefore the purification and removal of impurities becomes a key to the preparation of ultra-pure gases. The composite metal purifying agent used in the present market mainly uses metallic nickel as a main active component, and although impurities in gas can be removed at one time, the composite metal purifying agent has the problems of low adsorption capacity, high cost and the like.
The activated carbon is an adsorbent with good application prospect, is widely applied to the production and living fields of gas purification, water purification, odor removal, decoloration and the like due to the high specific surface area and rich pore structure, but the removal of impurity gas in the ultrapure gas is not reported.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a nickel-based purifying agent with high hydrogen absorption capacity, and a preparation method and application thereof.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
the nickel-based purifying agent comprises the following components in percentage by mass: 75-85 wt% of nickel oxide, 5-15 wt% of aluminum oxide, 1-5 wt% of rare earth metal oxide and 5-15 wt% of active carbon.
Preferably: 75-80 wt% of nickel oxide, 5-10 wt% of aluminum oxide, 4-5 wt% of rare earth metal oxide and 6-10 wt% of activated carbon.
The rare earth metal oxide is one of samarium oxide, lanthanum oxide, cerium oxide and praseodymium oxide.
The preparation method of the nickel-based purifying agent comprises the following steps: adding nickel salt and rare earth metal salt into deionized water for dissolving, adding an alumina precursor to obtain a mixed material, adding activated carbon into the mixed material, adding a precipitator for reaction to generate a precipitation product, performing suction filtration, washing, drying and roasting on the precipitation product to obtain a mixture of nickel oxide, alumina, rare earth metal oxide and activated carbon, and performing tabletting to obtain the nickel-based purifying agent, wherein the nickel-based purifying agent contains 75-85 wt% of nickel oxide, 5-15 wt% of alumina, 1-5 wt% of rare earth metal oxide and 5-15 wt% of activated carbon. Preferably 75-80 wt% of nickel oxide, 5-10 wt% of aluminum oxide, 4-5 wt% of rare earth metal oxide and 6-10 wt% of activated carbon.
The method specifically comprises the following steps:
crushing activated carbon into powder of 300-400 meshes, and drying at 80-120 ℃ for 6-12 hours for later use;
secondly, weighing a certain amount of nickel salt and rare earth metal salt respectively, adding a certain amount of deionized water for dissolving, and adding a certain amount of alumina precursor for fully stirring to prepare a mixed material;
adding activated carbon powder prepared in the step into the mixed material prepared in the step II, heating to 60-80 ℃, uniformly stirring, then dropwise adding a precipitant solution, controlling the pH value of the system to 8-10, and continuously stirring for 1-5 hours to generate a precipitation product;
fourthly, carrying out suction filtration on the precipitated product obtained in the step (3), washing to be neutral, drying in an oven at the temperature of 80-120 ℃ for 5-12 hours, and roasting in a nitrogen atmosphere at the temperature of 300-500 ℃ for 5-12 hours to obtain a mixture containing nickel oxide, aluminum oxide, rare earth metal oxide and active carbon;
and fifthly, crushing the mixture obtained by roasting in the step (4) into 200-300 meshes of powder, and tabletting and forming to obtain the nickel-based purifying agent.
The nickel salt is one of nickel nitrate, nickel sulfate and nickel chloride;
the rare earth metal salt is one of samarium nitrate, lanthanum nitrate, cerium nitrate and praseodymium nitrate;
the active carbon is coconut shell active carbon or coal-based active carbon.
The alumina precursor is one of pseudo-boehmite powder, activated alumina powder or aluminum nitrate.
The precipitator solution is one of a sodium hydroxide solution, a potassium hydroxide solution and a sodium carbonate solution, and the concentration of the precipitator solution is 1-3 mol/L.
The nickel-based purifying agent is used for adsorbing and removing hydrogen in inert gas.
The inert gas can be nitrogen, helium or argon.
Compared with the prior art, the invention has the following beneficial effects:
in order to obtain an ideal hydrogen adsorption effect, the components and the dosage are also screened, the result shows that the different components have obvious influence on the adsorption capacity of the purifying agent, and the content of each component has obvious influence on the adsorption capacity of the purifying agent, the invention selects specific components and contents, and the result shows that: the purifying agent comprises 75-80 wt% of nickel oxide, 5-10 wt% of alumina and 4-5 w% of rare earth metal oxidet%, 6-10 wt% of activated carbon, H2The adsorption capacity is optimal.
The purifying agent comprises nickel oxide, aluminum oxide, rare earth metal oxide and active carbon, and multiple components have synergistic effect, and the purifying agent obtained by compounding is used for adsorbing and removing hydrogen in nitrogen, has the characteristics of high hydrogen adsorption capacity, high dehydrogenation precision and long service life, can be repeatedly regenerated and used, and has the advantages of simple preparation process, low cost and good industrial application prospect.
Detailed Description
The following examples are presented to further illustrate embodiments of the present invention, and it should be understood that the embodiments described herein are for purposes of illustration and explanation only and are not intended to limit the invention.
Example 1
The nickel-based purifying agent comprises the following components in percentage by mass: 75 wt% of nickel oxide, 10 wt% of aluminum oxide, 5 wt% of lanthanum oxide and 10 wt% of activated carbon.
The preparation method of the nickel-based purifying agent comprises the following steps:
(1) preparing activated carbon from MHG1.5 coal produced by Ningxia sea blue Industrial & trade Co., Ltd, grinding and sieving the activated carbon to powder of 300-400 meshes, weighing 10g of the activated carbon, and drying the powder in an oven at 120 ℃ for 5 hours for later use;
(2) 292g of nickel nitrate and 6.7g of lanthanum nitrate are respectively weighed, 440g of deionized water is added for dissolution, 15g of pseudo-boehmite powder (the content of alumina is 66.7 percent) is added, and the mixture is fully stirred to prepare a mixed material;
(3) adding the activated carbon powder prepared in the step into the mixed material prepared in the step II, heating to 70 ℃, dripping 2.35mol/L sodium carbonate aqueous solution while stirring for precipitation until the pH value is 8.8, and continuously stirring for 2 hours at 70 ℃;
(4) carrying out suction filtration and washing on the precipitate in the step (3) to neutrality, drying the precipitate at 110 ℃ for 10 hours, and roasting the precipitate at 500 ℃ for 5 hours in a nitrogen atmosphere to obtain a mixture containing activated carbon, nickel oxide, aluminum oxide and lanthanum oxide;
(5) and (3) crushing, grinding and sieving the mixture obtained in the step (4) to obtain 200-300-mesh powder, and then tabletting and forming to obtain the nickel-based purifying agent, wherein the nickel-based purifying agent contains 75 wt% of nickel oxide, 10 wt% of aluminum oxide, 5 wt% of lanthanum oxide and 10 wt% of activated carbon.
Example 2
The nickel-based purifying agent comprises the following components in percentage by mass: 80 wt% of nickel oxide, 8 wt% of aluminum oxide, 4 wt% of samarium oxide and 8 wt% of activated carbon.
The preparation method of the nickel-based purifying agent comprises the following steps:
(1) grinding and sieving MHG1.5 coal-made active carbon to powder of 300-400 meshes, weighing 8g of the powder, and drying the powder in an oven at 120 ℃ for 5 hours for later use;
(2) respectively weighing 311g of nickel nitrate and 6.7g of samarium nitrate, adding 475g of deionized water for dissolving, adding 12g of pseudo-boehmite powder (wherein the content of alumina is 66.7 percent), and fully stirring to prepare a mixed material;
(3) adding the activated carbon powder prepared in the step into the mixed material prepared in the step II, heating to 70 ℃, dripping 2.35mol/L sodium carbonate aqueous solution while stirring for precipitation until the pH value is 8.8, and continuously stirring for 2 hours at 70 ℃;
(4) filtering and washing the precipitate in the step (3) to be neutral, drying the precipitate at 110 ℃ for 10 hours, and roasting the precipitate at 500 ℃ for 5 hours in a nitrogen atmosphere to obtain a mixture containing nickel oxide, aluminum oxide, samarium oxide and active carbon;
(5) and (3) crushing, grinding and sieving the mixture obtained in the step (4) to obtain 200-300-mesh powder, and then tabletting and forming to obtain the nickel-based purifying agent, wherein the nickel-based purifying agent contains 80 wt% of nickel oxide, 8 wt% of aluminum oxide, 4 wt% of samarium oxide and 8 wt% of activated carbon.
Example 3
The nickel-based purifying agent comprises the following components in percentage by mass: 85 wt% of nickel oxide, 5 wt% of aluminum oxide, 4 wt% of samarium oxide and 6 wt% of activated carbon.
The preparation method of the nickel-based purifying agent comprises the following steps:
(1) grinding and sieving MHG1.5 coal-made active carbon to powder of 300-400 meshes, weighing 6g of the powder, and drying the powder in an oven at 120 ℃ for 5 hours for later use;
(2) weighing 331g of nickel nitrate and 6.7g of samarium nitrate respectively, adding 500g of deionized water for dissolving, adding 7.5g of pseudo-boehmite powder (wherein the content of alumina is 66.7 percent), and fully stirring to prepare a mixed material;
(3) adding the activated carbon powder prepared in the step into the mixed material prepared in the step II, heating to 70 ℃, dripping 2.35mol/L sodium carbonate aqueous solution while stirring for precipitation until the pH value is 8.8, and continuously stirring for 2 hours at 70 ℃;
(4) filtering and washing the precipitate in the step (3) to be neutral, drying the precipitate at 110 ℃ for 10 hours, and roasting the precipitate at 500 ℃ for 5 hours in a nitrogen atmosphere to obtain a mixture containing nickel oxide, aluminum oxide, samarium oxide and active carbon;
(5) and (3) crushing, grinding and sieving the mixture obtained in the step (4) to obtain 200-300-mesh powder, and then tabletting and forming to obtain the nickel-based purifying agent, wherein the nickel-based purifying agent contains 85 wt% of nickel oxide, 5 wt% of aluminum oxide, 4 wt% of samarium oxide and 6 wt% of activated carbon.
Comparative example 1
The raw materials comprise 9g of active carbon prepared from MHG1.5 coal, 311g of nickel nitrate and 16.5g of pseudo-boehmite powder (wherein the content of alumina is 66.7 percent), and the preparation method is the same as that of the example 2, so that the nickel-based purifying agent containing 80 weight percent of nickel oxide, 11 weight percent of alumina and 9 weight percent of active carbon is obtained.
Comparative example 2
The raw materials comprise 311g of nickel nitrate, 6.7g of samarium nitrate and 24g of pseudo-boehmite powder (wherein the content of alumina is 66.7%), and the preparation method is the same as that in example 2, so that the nickel-based purifying agent containing 80 wt% of nickel oxide, 16 wt% of alumina and 4 wt% of samarium oxide is obtained.
Comparative example 3
The raw materials are 311g of nickel nitrate and 30g of pseudo-boehmite powder (the content of alumina is 66.7 percent), and the preparation method is the same as that of the example 2, so that the nickel-based purifying agent containing 80 weight percent of nickel oxide and 20 weight percent of alumina is obtained.
Comparative example 4
The raw materials comprise 20g of active carbon prepared from MHG1.5 coal, 253g of nickel nitrate, 13.3g of lanthanum nitrate and 7.5g of pseudo-boehmite powder (wherein the content of alumina is 66.7%), the amount of deionized water for dissolving the nickel nitrate and the lanthanum nitrate is 390g, and the preparation method is the same as that of the example 1, so that the nickel-based purifying agent containing 65 wt% of nickel oxide, 5 wt% of alumina, 10% of lanthanum oxide and 20% of active carbon is obtained.
Comparative example 5
2g of active carbon prepared from MHG1.5 coal, 350g of nickel nitrate, 4g of lanthanum nitrate, 7.5g of pseudo-boehmite powder (wherein the content of alumina is 66.7%), and 530g of deionized water for dissolving the nickel nitrate and the lanthanum nitrate.
Comparative example 6
(1) Grinding and sieving MHG1.5 coal-made active carbon to powder of 300-400 meshes, weighing 8g of the powder, and drying the powder in an oven at 120 ℃ for 5 hours for later use;
(2) respectively weighing 311g of nickel nitrate, 6.7g of samarium nitrate and 12g of pseudo-boehmite powder (wherein the content of alumina is 66.7 percent) to prepare a mixed material, and putting the mixed material into a muffle furnace to roast for 6 hours at 500 ℃;
(3) grinding and sieving a roasted product prepared in the step II to obtain 300-400 mesh powder;
(4) the method comprises the steps of adding the activated carbon powder prepared in the step one into the material powder prepared in the step three, fully mixing, and then performing tabletting and forming to obtain the nickel-based purifying agent, wherein the nickel-based purifying agent contains 80 wt% of nickel oxide, 8 wt% of aluminum oxide, 4 wt% of samarium oxide and 8 wt% of activated carbon.
The examples and comparative examples were subjected to a hydrogen adsorption removal experiment: crushing and screening the purifying agent to 20-30 meshes, taking 5ml of the purifying agent, and filling the purifying agent into a stainless steel reactor with the inner diameter of 12mm at an airspeed of 1000h-1Introducing high-purity hydrogen for pre-reduction, keeping the temperature at 100 ℃ for 1 hour, keeping the temperature at 300 ℃ for 3 hours, introducing a high-purity nitrogen replacement bed layer after the reduction is finished, cooling to room temperature, and then keeping the space velocity at 5000h-1Introducing nitrogen containing 500ppm hydrogen, detecting outlet hydrogen concentration on line, stopping reaction when outlet hydrogen concentration exceeds 0.01ppm, and calculating H of purifying agent2Adsorption capacity. The results are shown in Table 1.
Table 1: component content in each sample and its H2 adsorption capacity
O means that the purifying agent is prepared without the component
As can be seen from Table 1, H in examples 1 to 3 and comparative examples 1 to 32The adsorption capacity data show that different components in the sample have obvious influence on the adsorption capacity of the purifying agent, and the purifying agent does not contain rare earth elements or active carbon or comparative examples 1-3 containing neither rare earth elements or active carbon, and H is H2Adsorption capacities of 6.2, 5.8 and 5.0ml/g, respectively, for H in examples 1 to 3 of the present application2The adsorption capacity of the purifying agent is obviously higher than that of comparative examples 1-3, which shows that the purifying agent prepared by the method is prepared by the interaction of a plurality of components, the adsorption capacity of the purifying agent can be further improved by compounding, and all the components have synergistic effect and are absolutely absent.
From the H of examples 1 to 3 and comparative examples 4 to 5 in Table 12The adsorption capacity data show that the content of each component in the sample has obvious influence on the adsorption capacity of the purifying agent, and the content of each component is not in comparative examples 4-5 of the protection range, and H is2Adsorption capacities of 6.1 and 6.5ml/g, respectively, for H in examples 1 to 3 of the present application2The adsorption capacity is obviously higher than that of comparative examples 4-5, which shows that the specific component content of the adsorbent can achieve good adsorption effect.
From examples 1 to 3 and comparative example 6 in Table 1, H2The adsorption capacity data is visible, and the preparation method is used for H of the purifying agent2Adsorption Capacity had a significant impact, and H of comparative example 6, obtained by simple physical mixing of the components2The adsorption capacity was only 2.8ml/g, compared with that of H in examples 1 to 3 of the present application2The adsorption capacity is obviously higher than that of the comparative example 6, which shows that the components obtained by the preparation method of the application are uniformly distributed, thereby achieving good adsorption effect.
Claims (10)
1. A nickel-based purifying agent, which is characterized in that: the nickel-based purifying agent comprises the following components in percentage by mass: 75-85 wt% of nickel oxide, 5-15 wt% of aluminum oxide, 1-5 wt% of rare earth metal oxide and 5-15 wt% of active carbon.
2. The nickel-based scavenger according to claim 1, wherein: the nickel-based purifying agent comprises the following components in percentage by mass: 75-80 wt% of nickel oxide, 5-10 wt% of aluminum oxide, 4-5 wt% of rare earth metal oxide and 6-10 wt% of activated carbon.
3. The nickel-based scavenger according to claim 2, wherein: the rare earth metal oxide is one of samarium oxide, lanthanum oxide, cerium oxide and praseodymium oxide.
4. A preparation method of the nickel-based purifying agent as claimed in any one of claims 1 to 3, characterized in that after nickel salt and rare earth metal salt are added into deionized water for dissolution, alumina precursor is added to obtain a mixture, activated carbon is added into the mixture, a precipitator is added for reaction to generate a precipitation product, the precipitation product is filtered, washed, dried and roasted to obtain a mixture of nickel oxide, alumina, rare earth metal oxide and activated carbon, and the mixture is tableted and molded to obtain the nickel-based purifying agent.
5. The preparation method of the nickel-based purifying agent as described in claim 4, wherein the nickel-based purifying agent comprises the following components by mass percent: 75-85 wt% of nickel oxide, 5-15 wt% of aluminum oxide, 1-5 wt% of rare earth metal oxide and 5-15 wt% of active carbon.
6. The preparation method of the nickel-based purifying agent as claimed in claim 5, wherein the nickel-based purifying agent comprises the following components in percentage by mass: 75-80 wt% of nickel oxide, 5-10 wt% of aluminum oxide, 4-5 wt% of rare earth metal oxide and 6-10 wt% of activated carbon.
7. The method for preparing a nickel-based scavenger according to claim 4, comprising the steps of:
crushing activated carbon into powder of 300-400 meshes, and drying at 80-120 ℃ for 6-12 hours for later use;
adding deionized water into the nickel salt and the rare earth metal salt for dissolving, and adding an alumina precursor for fully stirring to prepare a mixed material;
adding activated carbon powder prepared in the step into the mixed material prepared in the step II, heating to 60-80 ℃, uniformly stirring, then dropwise adding a precipitant solution, controlling the pH value of the system to 8-10, and continuously stirring for 1-5 hours to generate a precipitation product;
fourthly, carrying out suction filtration on the precipitated product obtained in the step (3), washing to be neutral, drying in an oven at the temperature of 80-120 ℃ for 5-12 hours, and roasting in a nitrogen atmosphere at the temperature of 300-500 ℃ for 5-12 hours to obtain a mixture containing nickel oxide, aluminum oxide, rare earth metal oxide and active carbon;
and fifthly, crushing the mixture obtained by roasting in the step (4) into 200-300 meshes of powder, and tabletting and forming to obtain the nickel-based purifying agent.
8. The method for producing a nickel-based scavenger having a high hydrogen absorption capacity according to claim 4, wherein: the nickel salt is one of nickel nitrate, nickel sulfate and nickel chloride;
the rare earth metal salt is one of samarium nitrate, lanthanum nitrate, cerium nitrate and praseodymium nitrate;
the active carbon is coconut shell active carbon or coal-based active carbon.
The alumina precursor is one of pseudo-boehmite powder, activated alumina powder or aluminum nitrate.
9. The method for producing a nickel-based scavenger having a high hydrogen absorption capacity according to claim 4, wherein: the precipitator solution is one of a sodium hydroxide solution, a potassium hydroxide solution and a sodium carbonate solution, and the concentration of the precipitator solution is 1-3 mol/L.
10. Use of a nickel-based scavenger according to claim 1, wherein the nickel-based scavenger is used for the adsorptive removal of hydrogen from an inert gas.
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